CN107335345B - Self-supporting high-moisture-permeability heat-insulating aerogel film and preparation method thereof - Google Patents
Self-supporting high-moisture-permeability heat-insulating aerogel film and preparation method thereof Download PDFInfo
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- CN107335345B CN107335345B CN201710643131.5A CN201710643131A CN107335345B CN 107335345 B CN107335345 B CN 107335345B CN 201710643131 A CN201710643131 A CN 201710643131A CN 107335345 B CN107335345 B CN 107335345B
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- 239000004964 aerogel Substances 0.000 title claims abstract description 142
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 59
- 229920002678 cellulose Polymers 0.000 claims abstract description 20
- 239000001913 cellulose Substances 0.000 claims abstract description 20
- 239000002904 solvent Substances 0.000 claims abstract description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 7
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 6
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 6
- 239000002356 single layer Substances 0.000 claims abstract description 6
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 6
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 6
- 239000013354 porous framework Substances 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 126
- 239000012528 membrane Substances 0.000 claims description 44
- 238000000034 method Methods 0.000 claims description 39
- 238000002791 soaking Methods 0.000 claims description 36
- 239000011521 glass Substances 0.000 claims description 35
- 239000000758 substrate Substances 0.000 claims description 35
- 239000011248 coating agent Substances 0.000 claims description 34
- 238000000576 coating method Methods 0.000 claims description 34
- 239000008367 deionised water Substances 0.000 claims description 27
- 229910021641 deionized water Inorganic materials 0.000 claims description 27
- 230000007062 hydrolysis Effects 0.000 claims description 27
- 238000006460 hydrolysis reaction Methods 0.000 claims description 27
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N dimethyl sulfoxide Natural products CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 26
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 24
- 239000012510 hollow fiber Substances 0.000 claims description 23
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 22
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 22
- 239000003960 organic solvent Substances 0.000 claims description 20
- 229910052710 silicon Inorganic materials 0.000 claims description 20
- 239000010703 silicon Substances 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 19
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 19
- 238000003756 stirring Methods 0.000 claims description 19
- 229920001046 Nanocellulose Polymers 0.000 claims description 17
- 239000002253 acid Substances 0.000 claims description 17
- 238000001035 drying Methods 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 15
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 13
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 12
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 11
- 238000001879 gelation Methods 0.000 claims description 11
- 230000004048 modification Effects 0.000 claims description 11
- 238000012986 modification Methods 0.000 claims description 11
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 claims description 11
- 239000003921 oil Substances 0.000 claims description 11
- 229920001897 terpolymer Polymers 0.000 claims description 11
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 10
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Natural products CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 10
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 10
- 238000000502 dialysis Methods 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 9
- 239000000725 suspension Substances 0.000 claims description 9
- 229920000642 polymer Polymers 0.000 claims description 8
- 239000012153 distilled water Substances 0.000 claims description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical group CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 6
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical group C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 6
- 229940113088 dimethylacetamide Drugs 0.000 claims description 6
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims description 6
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000005096 rolling process Methods 0.000 claims description 6
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims description 6
- 239000005051 trimethylchlorosilane Substances 0.000 claims description 6
- RSIHJDGMBDPTIM-UHFFFAOYSA-N ethoxy(trimethyl)silane Chemical compound CCO[Si](C)(C)C RSIHJDGMBDPTIM-UHFFFAOYSA-N 0.000 claims description 4
- 235000019353 potassium silicate Nutrition 0.000 claims description 4
- DZSVIVLGBJKQAP-UHFFFAOYSA-N 1-(2-methyl-5-propan-2-ylcyclohex-2-en-1-yl)propan-1-one Chemical compound CCC(=O)C1CC(C(C)C)CC=C1C DZSVIVLGBJKQAP-UHFFFAOYSA-N 0.000 claims description 3
- 229920000875 Dissolving pulp Polymers 0.000 claims description 3
- 239000013078 crystal Substances 0.000 claims description 3
- 238000004108 freeze drying Methods 0.000 claims description 3
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 3
- 239000004115 Sodium Silicate Substances 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims description 2
- 238000007710 freezing Methods 0.000 claims description 2
- 230000008014 freezing Effects 0.000 claims description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 2
- 239000011148 porous material Substances 0.000 claims description 2
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 2
- 125000003944 tolyl group Chemical group 0.000 claims description 2
- 239000002131 composite material Substances 0.000 abstract description 14
- 239000007787 solid Substances 0.000 abstract description 14
- 230000003301 hydrolyzing effect Effects 0.000 abstract description 10
- 230000035699 permeability Effects 0.000 abstract description 10
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 230000008901 benefit Effects 0.000 abstract description 8
- 238000009413 insulation Methods 0.000 abstract description 8
- 239000000654 additive Substances 0.000 abstract description 3
- 230000000996 additive effect Effects 0.000 abstract description 3
- 231100000053 low toxicity Toxicity 0.000 abstract description 3
- 231100000252 nontoxic Toxicity 0.000 abstract description 3
- 230000003000 nontoxic effect Effects 0.000 abstract description 3
- 239000010408 film Substances 0.000 description 148
- 239000000243 solution Substances 0.000 description 65
- 238000007791 dehumidification Methods 0.000 description 37
- 239000013535 sea water Substances 0.000 description 31
- 238000010612 desalination reaction Methods 0.000 description 17
- 239000010409 thin film Substances 0.000 description 16
- 230000008569 process Effects 0.000 description 15
- 239000011259 mixed solution Substances 0.000 description 13
- 239000000084 colloidal system Substances 0.000 description 10
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 10
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 9
- 229920000536 2-Acrylamido-2-methylpropane sulfonic acid Polymers 0.000 description 8
- XHZPRMZZQOIPDS-UHFFFAOYSA-N 2-Methyl-2-[(1-oxo-2-propenyl)amino]-1-propanesulfonic acid Chemical compound OS(=O)(=O)CC(C)(C)NC(=O)C=C XHZPRMZZQOIPDS-UHFFFAOYSA-N 0.000 description 8
- 239000007888 film coating Substances 0.000 description 7
- 238000009501 film coating Methods 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 238000011049 filling Methods 0.000 description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000013505 freshwater Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 235000006408 oxalic acid Nutrition 0.000 description 3
- 238000001223 reverse osmosis Methods 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000011033 desalting Methods 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 229920006254 polymer film Polymers 0.000 description 2
- 239000008213 purified water Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 229920009405 Polyvinylidenefluoride (PVDF) Film Polymers 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
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- 230000000903 blocking effect Effects 0.000 description 1
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- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical group [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 239000002274 desiccant Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
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- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
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- 238000009210 therapy by ultrasound Methods 0.000 description 1
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/26—Drying gases or vapours
- B01D53/268—Drying gases or vapours by diffusion
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
- B01D61/025—Reverse osmosis; Hyperfiltration
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- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01D69/08—Hollow fibre membranes
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- B01D71/06—Organic material
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- B01D71/10—Cellulose; Modified cellulose
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D71/06—Organic material
- B01D71/70—Polymers having silicon in the main chain, with or without sulfur, nitrogen, oxygen or carbon only
- B01D71/702—Polysilsesquioxanes or combination of silica with bridging organosilane groups
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- B01D71/82—Macromolecular material not specifically provided for in a single one of groups B01D71/08 - B01D71/74 characterised by the presence of specified groups, e.g. introduced by chemical after-treatment
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
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- C02F1/441—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by reverse osmosis
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D71/06—Organic material
- B01D71/40—Polymers of unsaturated acids or derivatives thereof, e.g. salts, amides, imides, nitriles, anhydrides, esters
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/448—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by pervaporation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/08—Seawater, e.g. for desalination
Abstract
The invention discloses a self-supporting high-moisture-permeability heat-insulating aerogel film and a preparation method thereof. The aerogel film is SiO2The self-supporting single-layer film with the porous framework structure is 150-300 mu m thick, has the advantages of high moisture permeability, high permselectivity, high strength, thermal insulation and high porosity, and has the advantages that the exchange rate of water vapor is increased by 50-200% and the thermal conductivity coefficient is reduced by 50-90% compared with the traditional solid composite film. The preparation method comprises the following steps: (1) preparing a template; (2) hydrolyzing the nano-cellulose; (3) preparing an aerogel film; (4) and (4) carrying out aftertreatment on the aerogel film. The preparation method is simple and easy to operate, adopts low-toxicity solvent and non-toxic additive, and has the advantages of environment-friendly production process, low equipment requirement, good film forming property and low production cost.
Description
Technical Field
The invention relates to the technical field of preparation of membranes used for water treatment and air dehumidification, in particular to a self-supporting high-moisture-permeability heat-insulating aerogel thin film and a preparation method thereof.
Background
Fresh water resources are one of the most important material bases for human survival and development. Sea water desalination and wastewater purification technologies are becoming important means to solve the shortage of fresh water resources.
Desalination of sea water, also known as sea water desalination, is a process of separating salt and water from sea water. The commonly used seawater desalination methods include a thermal method and a membrane method. The thermal method mainly adopts multi-stage flash evaporation, multi-effect distillation and vapor compression distillation; the membrane process is mainly reverse osmosis. Thermal processes typically consume large amounts of high grade energy and the production equipment is complex and expensive; the reverse osmosis technology of membrane process is a technology which utilizes the selective permeability of semipermeable membrane, under the condition of external high pressure makes water pass through the semipermeable membrane in reverse concentration gradient, and makes salt and impurity be retained on another side of membrane. The reverse osmosis method is generally driven by electric energy and mechanical energy, a system needs to maintain higher operating pressure, and the requirement on the pressure resistance of equipment is high. The existing hot method and membrane method seawater desalination technologies have the problems of high equipment requirement, large consumption of high-grade energy and low fresh water yield of seawater.
Meanwhile, people pay more and more attention to improvement of indoor environment. The dehumidification method can be classified into: cooling dehumidification, desiccant dehumidification (including liquid absorption dehumidification and solid adsorption dehumidification), membrane permeation dehumidification, electrochemical dehumidification and the like. The cooling dehumidification method utilizes a cooling coil to reduce the temperature of air to be below the dew point temperature of the air, so that moisture in the air is condensed and condensed on the surface of a cooler. The membrane permeation dehumidification method is a method for dehumidifying air on the high water vapor partial pressure side by transferring water from the side with high water vapor partial pressure to the side with low water vapor partial pressure by utilizing the selective permeability of a membrane to water in the air. The electrochemical dehumidification method is to decompose water vapor into oxygen and protons at the anode of the battery, and then transfer the protons to the cathode to generate hydrogen molecules or combine the hydrogen molecules with oxygen to generate water, so as to reduce the moisture in the air.
The above-mentioned cooling dehumidification, membrane permeation dehumidification and electrochemical dehumidification methods all have significant drawbacks. The cooling dehumidification method needs to cool the temperature of the air to be below the dew point of the air, the cooled air can be sent into a room after being heated again, and the temperature and the humidity can not be independently controlled in the process, so that the energy utilization rate is low, and the energy consumption is high; moisture is condensed on the surface of the cooler, so that the cooler is wet all the year round, a growing and multiplying place is provided for bacteria, and the indoor air quality is seriously reduced; in the case of the working condition that the dew point temperature is too low, the surface of the cooler is easy to frost, and a special device is needed for defrosting the cooler. The membrane method dehumidification is a passive dehumidification method, and the dehumidification capacity of the membrane method dehumidification is controlled by one side with lower water vapor pressure in the moisture exchange gas; the membrane material is an important factor influencing the dehumidification of the membrane method, and the performance of the whole dehumidification process is determined by the quality of the membrane material. Electrochemical dehumidification is a very novel dehumidification method, and the technology is not mature enough; in addition, a direct-current power supply is needed in the dehumidification process, and the energy utilization is not high.
The existing membrane has the defects that the contradiction between high moisture permeability and the barrier to the permeation of other gas molecules is difficult to satisfy simultaneously, the energy loss caused by the overhigh heat conductivity coefficient of the membrane material is overlarge, the preparation cost is overhigh, and the used material is not environment-friendly.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a self-supporting high-moisture-permeability heat-insulating aerogel film. The self-supporting high-moisture-permeability heat-insulating aerogel film can be used for realizing independent dehumidification of air or seawater desalination; used for independent dehumidification of air, can realize high moisture permeability, high mechanical strength and extremely low heat conductivity coefficient of air, and is suitable for the treatment of the diseases including N2Other gas molecules have strong blocking effect and can reduce the sensible heat transfer in the process; the composite material is used for seawater desalination, has high selective permeability, can reduce equipment requirements and energy consumption, and improves the seawater desalination yield.
The invention also aims to provide a preparation method of the self-supporting high-moisture-permeability heat-insulating aerogel film. The method adopts low-toxicity solvent and nontoxic additive, and has the advantages of environment-friendly production process, simple process and low production cost.
The purpose of the invention is realized by the following technical scheme.
A preparation method of a self-supporting high moisture-permeable heat-insulating aerogel film comprises the following steps:
(1) preparing a template: cleaning the glass substrate, and removing oil stains on the surface; filtering the solution of the high molecular polymer by microporous filter paper, and coating the solution on a glass substrate to obtain a template for later use;
(2) hydrolysis of nanocellulose: uniformly dispersing the nano cellulose whiskers in an organic solvent under heating and stirring, and then adding a silicon source, acid and deionized water for hydrolysis;
(3) preparing an aerogel film: after the hydrolysis is finished, standing, adding gel liquid for gelation, coating the obtained gel on one side of the template with the high molecular polymer to form an aerogel film, quickly soaking the aerogel film in a solvent, and taking out the aerogel film to obtain the template loaded with the aerogel film;
(4) and (3) carrying out aftertreatment on the aerogel film: and (2) carrying out solvent exchange and surface modification on the template loaded with the aerogel film, drying, stripping from the glass substrate to obtain the aerogel film, and roasting at high temperature to obtain the self-supporting high-moisture-permeability heat-insulating aerogel film.
Further, in the step (1), the glass substrate is sequentially soaked in ethanol, acetone and deionized water for ultrasonic treatment for 20-40 min.
Further, in the step (1), the high molecular polymer comprises acrylamide/2-acrylamido-2-methylpropanesulfonic acid terpolymer (PAMS).
Further, in the step (1), the mass concentration of the solution of the high molecular polymer is 10-20 wt.%.
Further, in the step (1), the pore size of the microporous filter paper is 30-50 μm, and the polymer fiber residue with large particle size is removed by filtering through the microporous filter paper.
Further, in the step (2), the nano-cellulose whisker is prepared by the following method:
dissolving cellulose powder in concentrated sulfuric acid under heating and stirring, cooling to room temperature, and centrifugally washing with distilled water to obtain a non-stratified milky suspension; and dialyzing and separating the obtained milky suspension, and washing, freezing and drying the obtained crystal to obtain the nano cellulose whisker.
Further, the heating and stirring are carried out at 60-80 ℃.
Furthermore, the concentration of the concentrated sulfuric acid is 50-70 wt.%.
Further, the cooling to room temperature is carried out by directly adding distilled water.
Further, the dialysis is carried out by filling the milky suspension obtained by centrifugation into a cellulose dialysis bag and dialyzing the milky suspension in deionized water until the pH of the dialysate reaches 7.0.
Further, the freeze drying is carried out at-30 to-50 ℃.
Further, in the step (2), the silicon source includes one of methyl orthosilicate (TMOS), tetraethyl orthosilicate (TEOS), methyltrimethoxysilane, water glass, trimethylethoxysilane and silsesquioxane.
Further, in the step (2), the organic solvent is added according to the difference of the silicon source: when the silicon source is methyl orthosilicate, the organic solvent is dimethyl sulfoxide (DMSO); when the silicon source is tetraethoxysilane, the organic solvent is ethanol; when the silicon source is methyltrimethoxysilane, the organic solvent is tetrahydrofuran; when the silicon source is sodium silicate, the organic solvent is toluene; the silicon source is trimethyl ethoxy silane or silsesquioxane, and the organic solvent is dimethyl acetamide.
Further, in the step (2), the solid-to-liquid ratio of the nano cellulose whisker to the organic solvent is 5-10: 80-100 g/mL.
Further, in the step (2), the mass ratio of the organic solvent to the silicon source is 0.8-1.5: 0.3 to 0.6.
Further, in the step (2), the volume ratio of the organic solvent to the deionized water is 30-50: 2 to 4.
Further, in the step (2), the acid is added in an amount such that the molar ratio of the hydrogen atoms in the acid to the silicon atoms in the silicon source is 10-5~10-3: 1-3, and the pH of the solution after the acid is added is 5-6.
Further, in the step (2), the heating and stirring are performed at 40-80 ℃.
Further, in the step (2), the hydrolysis temperature is 40-80 ℃, and the hydrolysis time is 6-12 hours.
Further, in the step (3), the standing time is 24-48 h.
Further, in the step (3), the gel liquid includes one or more of ammonia water, ethanol, dimethyl sulfoxide and hexamethyldisilazane.
Further, in the step (3), the gel is prepared by adding gel liquid to make the colloid viscosity reach 7-20 cP.
Further, in the step (3), the solvent includes one or more of ethanol, ethyl orthosilicate and dimethyl sulfoxide.
Further, in the step (3), the soaking time is 24-72 hours, and the solvent is replaced every 8-16 hours.
Further, in the step (4), one of dimethyl sulfoxide, n-hexane, n-heptane and n-butane is adopted to replace the solvent adopted in the step (3) soaking in the silica sol at a constant temperature of 40-60 ℃, and then the solution of Trimethylchlorosilane (TMCS) is used for soaking for 24-48h for surface modification.
Furthermore, the solvent of the solution of the trimethylchlorosilane is one of n-hexane, n-heptane and n-butane, wherein the volume ratio of the trimethylchlorosilane to the solvent is 1: 9-15.
Further, in the step (4), the drying is carried out at the temperature of 80-120 ℃ and under normal pressure for 24-48 h.
Further, in the step (4), the high-temperature roasting temperature is 350-450 ℃, and the time is 4-8 hours.
Further, in the steps (1) and (3), the coating is performed by manually scraping the film by using a scraper or coating the film by using a mechanical film coating machine.
The self-supporting high-moisture-permeability heat-insulating aerogel film prepared by the preparation method is SiO2The thickness of the self-supporting single-layer film with the porous framework structure is 150-300 mu m; the SiO2The porous skeleton structure is a three-dimensional network structure; and (3) completely removing the calcined polymer film, and excluding the polymer film formed in the step (1) from the finally obtained self-supporting high-moisture-permeability heat-insulating aerogel film.
Further, the self-supporting high moisture-permeable heat-insulating aerogel thin film comprises two film types, namely a flat plate film and a hollow fiber film; the hollow fiber membrane is formed by rolling the flat membrane.
The flat membrane has large relative unit membrane area flux and good pollution resistance; the hollow fiber membrane has large filling density per unit volume of membrane area and low manufacturing cost.
Furthermore, the thermal conductivity coefficient of the self-supporting high moisture-permeable heat-insulating aerogel film is 0.02-0.03W/(mK).
The self-supporting high moisture permeable heat insulation aerogel film can be used for realizing independent dehumidification of air or seawater desalination.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the self-supporting high-moisture-permeability heat-insulation aerogel film has high moisture permeability and high selective permeability, and the exchange rate of water vapor is improved by 50-200% compared with that of the traditional solid composite film under the same experimental conditions;
(2) the self-supporting high-moisture-permeability heat-insulating aerogel film has high strength, and the nano-cellulose whiskers are contained in the film, so that the mechanical property of the aerogel film is greatly enhanced;
(3) the self-supporting high-moisture-permeability heat-insulation aerogel disclosed by the invention has good heat insulation performance, the silicon dioxide aerogel is a low-heat-conduction material, and is prepared into a film form under appropriate viscosity, so that the heat conductivity coefficient of the film can be greatly reduced, the heat conductivity coefficient of the film obtained by measurement is 0.02-0.03W/(mK), the heat conductivity coefficient is 50% -90% lower than that of the traditional solid composite film, and the heat conductivity coefficient is 82.3% -88.2% lower than that of a common polyvinylidene fluoride (PVDF) film (0.17W/(mK)), so that the practical application significance is great;
(4) the self-supporting high-moisture-permeability heat-insulating aerogel film has the advantage of extremely high porosity, and the porosity reaches 80-95%;
(5) the preparation method is simple and easy to operate, adopts low-toxicity solvent and non-toxic additive, and has the advantages of environment-friendly production process, low equipment requirement, good film forming property and low production cost.
Drawings
FIG. 1 is a schematic structural view of a flat sheet film type of the self-supporting high moisture permeable insulating aerogel thin film of the present invention;
FIG. 2 is a schematic structural view of a hollow fiber membrane type of the self-supporting high moisture permeable insulating aerogel film of the present invention;
FIG. 3 is a schematic structural view of a flat sheet membrane of the self-supporting high moisture permeable insulating aerogel thin film shown in FIG. 1 for use in a dehumidifier and a desalinator;
FIG. 4 is a schematic structural view of the hollow fiber membrane of the self-supporting high moisture permeable insulating aerogel film shown in FIG. 2 used in a dehumidifier and a seawater desalination plant.
Detailed Description
For a better understanding of the present invention, the present invention is described in further detail below with reference to specific examples and drawings, but the embodiments of the present invention are not limited thereto and may be performed with reference to the conventional art for process parameters not particularly noted.
The structural schematic diagrams of the single-layer film flat plate film type and the hollow fiber film type of the self-supporting high-moisture-permeability heat-insulating aerogel thin film are respectively shown in fig. 1 and fig. 2, and both have SiO2The thickness of the single-layer film of the porous supporting framework is 150-300 mu m; the single-layer porous scaffold of the flat membrane 1 shown in figure 1 and the hollow fiber membrane 2 shown in figure 2 are both three-dimensional net structures; the flat membrane 1 has large unit membrane area flux and good pollution resistance; the hollow fiber membrane 2 is formed by rolling the flat membrane 1, the filling density of the membrane area per unit volume is high, and the manufacturing cost is low;
the flat membrane is used for independent dehumidification of air and seawater desalination:
the structural schematic diagram of the self-supporting high moisture-permeable heat-insulating aerogel film used for the independent air dehumidifier and the seawater desalination device is shown in fig. 3, the independent air dehumidifier and the seawater desalination device are both cores of the flat film, and the flat film is made into the self-supporting high moisture-permeable heat-insulating aerogel bottom film with the same size as the bottom surface of the core; the core body comprises a solution channel inlet 3, a solution channel outlet 4, an air channel inlet 5, an air channel outlet 6 and a self-supporting high-moisture-permeability heat-insulating aerogel base membrane 7; the core body is a tetragonal core body formed by alternately stacking solution channels and air channels, solution channel inlets 3 and air channel inlets 5 are respectively arranged on two adjacent side faces, solution channel outlets 4 and air channel outlets 6 are respectively arranged on the other two adjacent side faces of the tetrahedron, the solution channel inlets 3 and the solution channel outlets 4 are communicated and are arranged on opposite side faces, and the air channel inlets 5 and the air channel outlets 6 are communicated and are arranged on opposite side faces, so that the solution and the air form cross flow in the working process; the solution channel and the air channel are stacked by adopting a bottom film 7 for separation, and the upper bottom and the lower bottom of the solution channel and the air channel are both self-supporting high-moisture-permeability heat-insulation aerogel bottom films 7.
The core body is used in the working process of independent dehumidification of air, a dehumidification solution enters the solution channel from the solution channel inlet 3, high-temperature and high-humidity outdoor air enters the air channel from the air channel inlet 5, the dehumidification solution and the outdoor air form cross flow, and heat and moisture exchange is completed in the core body; the low-humidity air after heat and humidity exchange is discharged from an air channel outlet 6, and the dehumidifying solution after heat and humidity exchange is discharged from a solution channel outlet 4, so that the aim of independently adjusting the indoor air humidity is fulfilled;
when the core body is used for desalting seawater, heated seawater enters the solution channel from the solution channel inlet 3, air enters the air channel from the air channel inlet 5, and the heated seawater and the air form cross flow; in the core body, the heated seawater humidifies the air to obtain high-humidity air; the desalinated seawater is discharged from the solution channel outlet 4, and the humidified air is discharged from the air channel 6 and passes through the water-cooling heat exchanger to precipitate purified water, so that the aim of desalinating seawater is fulfilled.
The hollow fiber membrane is used for independent dehumidification of air and desalination of sea water:
the structural schematic diagram of the self-supporting high moisture permeable heat insulation aerogel film of the invention used for the independent air dehumidifier and the seawater desalination device is shown in fig. 4, wherein the independent air dehumidifier and the seawater desalination device are both shells with closed upper and lower bottom surfaces and unsealed peripheral side surfaces; the flat membrane is rolled into a hollow fiber membrane tube 8, a plurality of hollow fiber membrane tubes 8 are assembled into a tube bundle with gaps, two ends of the tube bundle are respectively fixed on the shell, and the end openings of the hollow fiber tubes 8 are not closed, so that the hollow fiber tubes 8 are used as solution channels; one port of the hollow fiber tube 8 is a solution channel inlet 3, and the other port is a solution outlet 4; the unclosed side adjacent to the solution channel inlet 3 is an air channel inlet 5, and the other unclosed side opposite to the air channel inlet 5 is an air channel outlet 6; after entering the shell, the air and the solution form cross flow;
when the shell is used for independent air dehumidification, a dehumidification solution enters a solution channel formed by the hollow fiber tubes 8 from the solution channel inlet 3, high-temperature and high-humidity outdoor air enters the shell from the side surface adjacent to the solution channel inlet 3, namely the air channel inlet 5, and the outdoor air and the dehumidification solution form cross flow to perform heat and moisture exchange; the low-humidity air obtained after heat and humidity exchange is discharged from an air channel outlet 6, and the dehumidification solution after heat and humidity exchange is discharged from a solution channel outlet 4, so that the aim of independently adjusting the indoor air humidity is fulfilled;
in the working process of the shell for desalting seawater, heated seawater enters the hollow cellulose tube 8 from the solution channel inlet 3, air enters the shell from the air channel inlet 5, and the heated seawater and the air form cross flow; in the shell, the heated seawater humidifies the air to obtain high-humidity air; the desalinated seawater is discharged from the solution channel outlet 4, and the humidified air is discharged from the air channel 6 and passes through the water-cooling heat exchanger to precipitate purified water, so that the aim of desalinating seawater is fulfilled.
The nano-cellulose whisker in the specific embodiment of the invention is prepared by the following method, which specifically comprises the following steps:
dissolving cellulose powder in concentrated sulfuric acid with the concentration of 50-70 wt.% while heating and stirring at the temperature of 60-80 ℃, adding distilled water for cooling to room temperature, and centrifugally washing with the distilled water to obtain a non-stratified milky suspension; and filling the obtained milky suspension into a cellulose dialysis bag, putting the cellulose dialysis bag into deionized water for dialysis until the pH value of the dialysate reaches 7.0, washing the obtained crystal by distilled water, and carrying out freeze drying at-30 to-50 ℃ to obtain the nano cellulose whisker.
Example 1
(1) Preparing a template: sequentially soaking a glass substrate in ethanol, acetone and deionized water, respectively ultrasonically washing for 20min, removing surface oil stains, filtering a solution of 10wt.% acrylamide/2-acrylamido-2-methylpropanesulfonic acid terpolymer (PAMS) through microporous filter paper with the aperture of 30-50 mu m, coating the solution on the glass substrate, and obtaining a template with the coating thickness of 150 mu m for later use;
(2) hydrolysis of nanocellulose: uniformly dispersing 5g of nano-cellulose whiskers in 100mL of dimethyl sulfoxide under heating and stirring at 50 ℃, adding 22.4mL of methyl orthosilicate, 0.1mL of hydrochloric acid with the concentration of 0.1mol/L and 2mL of deionized water, adding acid, adjusting the pH of the solution to 5, and hydrolyzing at 50 ℃ for 6 hours;
(3) preparing an aerogel film: after the hydrolysis is finished, standing for 24h, adding 1mL of ammonia water with the concentration of 0.357mol/L and 32.15mL of dimethyl sulfoxide for gelation, enabling the colloid viscosity to reach 7cP, coating the obtained gel on one side of the template with the PAMS to form an aerogel film with the thickness of 150 micrometers, quickly soaking in ethanol for 24h, replacing the ethanol for 3 times during the process, and taking out to obtain the template loaded with the aerogel film;
(4) and (3) carrying out aftertreatment on the aerogel film: the template loaded with the aerogel film is subjected to dimethyl sulfoxide solvent to replace ethanol in silica sol at the constant temperature of 60 ℃, and then the volume ratio of TMCS: n-hexane = 1: and (3) soaking the mixed solution of 9 for 24 hours for surface modification, drying at 100 ℃ and normal pressure for 48 hours, stripping from the glass substrate to obtain an aerogel film, and roasting at 350 ℃ for 4 hours to obtain the self-supporting high-moisture-permeability heat-insulating aerogel film.
The prepared self-supporting high-moisture-permeability heat-insulating aerogel thin film is 150 mu m thick, is a flat film, has the heat conductivity coefficient of 0.025W/(mK), the porosity of 90 percent, the tensile strength of 1.7MPa and the exchange efficiency of water vapor of 80 percent, and is improved by 100 percent compared with the traditional solid composite film (40 percent).
Example 2
(1) Preparing a template: sequentially soaking a glass substrate in ethanol, acetone and deionized water, respectively ultrasonically washing for 40min, removing surface oil stains, filtering a 20wt.% solution of acrylamide/2-acrylamido-2-methylpropanesulfonic acid terpolymer (PAMS) through microporous filter paper with the aperture of 30-50 mu m, coating the solution on the glass substrate, and obtaining a template with the coating thickness of 200 mu m for later use;
(2) hydrolysis of nanocellulose: uniformly dispersing 3g of nano-cellulose whiskers in 50mL of ethanol under heating and stirring at 50 ℃, then adding 27.2mL of ethyl orthosilicate, 1mL of oxalic acid with the concentration of 0.1mol/L and 4mL of deionized water, adding acid, then adjusting the pH of the solution to 5.5, and hydrolyzing for 12h at 50 ℃;
(3) preparing an aerogel film: after the hydrolysis is finished, standing for 24h, adding 0.5mL of concentrated ammonia water with the concentration of 10mol/L and 10mL of ethanol for gelation to enable the colloid viscosity to reach 10cP, coating the obtained gel on one side of the template with the PAMS to form an aerogel film with the thickness of 200 micrometers, quickly soaking the aerogel film in dimethyl sulfoxide for 24h, replacing the dimethyl sulfoxide for 3 times during the process, and taking out to obtain the template loaded with the aerogel film;
(4) and (3) carrying out aftertreatment on the aerogel film: the template loaded with the aerogel film is subjected to normal hexane to replace ethanol in silica sol at the constant temperature of 40 ℃, and then TMCS (thermal mechanical control system) is adopted: n-hexane = 1: and (3) soaking the mixed solution of 10 for 32h for surface modification, drying at 80 ℃ for 48h under normal pressure, stripping from the glass substrate to obtain an aerogel film, and roasting at 450 ℃ for 8h to obtain the self-supporting high-moisture-permeability heat-insulating aerogel film.
The prepared self-supporting high-moisture-permeability heat-insulating aerogel thin film is 200 mu m thick and is a flat film, a hollow fiber film is formed by rolling, the heat conductivity coefficient of the hollow fiber film is 0.02W/(mK), the porosity is 95%, the strength is 1.3MPa, the exchange rate of water vapor is 120%, and the heat conductivity is improved by 200% compared with that of the traditional solid composite film (40%).
Example 3
(1) Preparing a template: sequentially soaking a glass substrate in ethanol, acetone and deionized water, respectively ultrasonically washing for 30min, removing surface oil stains, filtering a solution of acrylamide/2-acrylamido-2-methylpropanesulfonic acid terpolymer (PAMS) with the concentration of 15wt.% by microporous filter paper with the aperture of 30-50 mu m, and coating the solution on the glass substrate with the coating thickness of 300 mu m to obtain a template for later use;
(2) hydrolysis of nanocellulose: heating and stirring at 80 ℃, uniformly dispersing 10g of nano-cellulose whiskers in 90mL of tetrahydrofuran, then adding 18.2mL of methyltrimethoxysilane, 0.5mL of phosphoric acid with the concentration of 0.1mol/L and 3mL of deionized water, adding acid, then regulating the pH value of the solution to 6, and hydrolyzing at 50 ℃ for 8 hours;
(3) preparing an aerogel film: after the hydrolysis is finished, standing for 48h, adding 5ml of hexamethyldisilazane for gelation to enable the colloid viscosity to reach 8cP, coating the obtained gel on one side of the template with the PAMS by using a mechanical film coating machine to form an aerogel film with the thickness of 200 micrometers, rapidly soaking the aerogel film in ethanol for 24h, replacing the ethanol for 3 times during the period, and taking out to obtain the template loaded with the aerogel film;
(4) and (3) carrying out aftertreatment on the aerogel film: and (2) replacing ethanol in silica sol by using the template loaded with the aerogel film through n-heptane at the constant temperature of 50 ℃, and then using TMCS: n-heptane = 1: 15 for 48 hours, drying at 120 ℃ under normal pressure for 48 hours, stripping from the glass substrate to obtain an aerogel film, and roasting at 350 ℃ for 4 hours to obtain the self-supporting high-moisture-permeability heat-insulating aerogel film.
The prepared self-supporting high-moisture-permeability heat-insulating aerogel thin film is 300 mu m in thickness, is a flat film, has the heat conductivity coefficient of 0.03W/(mK), the porosity of 80 percent, the strength of 2.0MPa and the exchange efficiency of water vapor of 60 percent, and is improved by 50 percent compared with the traditional solid composite film (40 percent).
Example 4
(1) Preparing a template: sequentially soaking a glass substrate in ethanol, acetone and deionized water, respectively ultrasonically washing for 20min, removing surface oil stains, filtering a solution of acrylamide/2-acrylamido-2-methylpropanesulfonic acid terpolymer (PAMS) with the concentration of 15wt.% by microporous filter paper with the aperture of 30-50 mu m, and coating the solution on the glass substrate with the coating thickness of 200 mu m to obtain a template for later use;
(2) hydrolysis of nanocellulose: uniformly dispersing 10g of nano-cellulose whiskers in 100mL of toluene under heating and stirring at 40 ℃, adding 30.12mL of water glass (pure substance), 0.01mL of 2mol/L phosphoric acid and 3mL of deionized water, adding acid, adjusting the pH of the solution to 5.5, and hydrolyzing at 50 ℃ for 8 hours;
(3) preparing an aerogel film: after the hydrolysis is finished, standing for 48h, adding 0.5mL of concentrated ammonia water with the concentration of 10mol/L and 46.12mL of ethanol for gelation to enable the colloid viscosity to reach 10cP, coating the obtained gel on one side of the template with the PAMS by using a mechanical film coating machine to form an aerogel film with the thickness of 150 micrometers, quickly soaking the aerogel film in a mixed solution (4: 1 v/v) of ethanol and ethyl orthosilicate for 24h, changing the mixed solution for 3 times during the soaking, and taking out to obtain the template loaded with the aerogel film;
(4) and (3) carrying out aftertreatment on the aerogel film: and (2) replacing ethanol in silica sol by using the template loaded with the aerogel film through n-heptane at the constant temperature of 40 ℃, and then using TMCS: n-heptane = 1: and (3) soaking the mixed solution of 9 for 24 hours for surface modification, drying at 120 ℃ under normal pressure for 48 hours, stripping from the glass substrate to obtain an aerogel film, and roasting at 350 ℃ for 4 hours to obtain the self-supporting high-moisture-permeability heat-insulating aerogel film.
The obtained self-supporting high-moisture-permeability heat-insulating aerogel thin film is 200 mu m thick and is a flat film, a hollow fiber film is formed by rolling, the heat conductivity coefficient of the hollow fiber film is 0.0289W/(mK), the porosity is 85 percent, the strength is 1.8MPa, the exchange efficiency of water vapor is 100 percent, and the heat conductivity is improved by 150 percent compared with the traditional solid composite film (40 percent).
Example 5
(1) Preparing a template: sequentially soaking a glass substrate in ethanol, acetone and deionized water, respectively ultrasonically washing for 40min, removing surface oil stains, filtering a solution of acrylamide/2-acrylamide-2-methylpropanesulfonic acid terpolymer (PAMS) with the concentration of 18wt.% by microporous filter paper with the aperture of 30-50 mu m, coating the solution on the glass substrate, and obtaining a template with the coating thickness of 200 mu m for later use;
(2) hydrolysis of nanocellulose: uniformly dispersing 10g of nano-cellulose whiskers in 90mL of toluene under heating and stirring at 40 ℃, adding 27.82mL of water glass, 0.05mL of phosphoric acid with the concentration of 0.5mol/L and 2mL of deionized water, adding acid, adjusting the pH of the solution to 6, and hydrolyzing at 50 ℃ for 10 hours;
(3) preparing an aerogel film: after the hydrolysis is finished, standing for 48h, adding 0.3mL of concentrated ammonia water with the concentration of 10mol/L and 56.84mL of ethanol for gelation to enable the colloid viscosity to reach 8cP, coating the obtained gel on one side of the template with the PAMS by using a mechanical coating machine to form an aerogel film with the thickness of 300 micrometers, quickly soaking the aerogel film in tetraethoxysilane for 48h, replacing the tetraethoxysilane for 3 times during the period, and taking out to obtain the template loaded with the aerogel film;
(4) and (3) carrying out aftertreatment on the aerogel film: the template loaded with the aerogel film is subjected to n-butane to replace ethanol in silica sol at the constant temperature of 40 ℃, and then the volume ratio of TMCS: n-butane = 1: and (3) soaking the mixed solution of 9 for 24 hours for surface modification, drying at 80 ℃ under normal pressure for 48 hours, stripping from the glass substrate to obtain an aerogel film, and roasting at 350 ℃ for 4 hours to obtain the self-supporting high-moisture-permeability heat-insulating aerogel film.
The obtained self-supporting high-moisture-permeability heat-insulating aerogel thin film is 150 mu m thick, is a flat film, has the heat conductivity coefficient of 0.027W/(mK), the porosity of 90 percent, the strength of 1.9MPa and the exchange efficiency of water vapor of 90 percent, and is improved by 125 percent compared with the traditional solid composite film (40 percent).
Example 6
(1) Preparing a template: sequentially soaking a glass substrate in ethanol, acetone and deionized water, respectively ultrasonically washing for 25min, removing surface oil stains, filtering a 12wt.% solution of acrylamide/2-acrylamido-2-methylpropanesulfonic acid terpolymer (PAMS) through microporous filter paper with the aperture of 30-50 mu m, coating the solution on the glass substrate, and obtaining a template with the coating thickness of 250 mu m for later use;
(2) hydrolysis of nanocellulose: uniformly dispersing 8g of nano-cellulose whiskers in 92mL of dimethylacetamide while heating and stirring at 40 ℃, adding 22.4mL of methyltriethoxysilane, 2mL of hydrochloric acid with the concentration of 0.05mol/L and 3.5mL of deionized water, adding acid, adjusting the pH of the solution to 5, and hydrolyzing at 50 ℃ for 8 hours;
(3) preparing an aerogel film: after the hydrolysis is finished, standing for 24h, adding 0.6ml of 10mol/L concentrated ammonia water for gelation to enable the colloid viscosity to reach 9cP, coating the obtained gel on one side of the template with the PAMS by using a mechanical film coating machine to form an aerogel film with the thickness of 200 micrometers, quickly soaking the aerogel film in ethanol for 48h, replacing the ethanol for 3 times during the period, and taking out to obtain the template loaded with the aerogel film;
(4) and (3) carrying out aftertreatment on the aerogel film: the template loaded with the aerogel film is subjected to normal butane to replace ethanol in silica sol at the constant temperature of 50 ℃, and then the volume ratio of TMCS: n-butane = 1: and (3) soaking the mixed solution of 9 for 32 hours for surface modification, drying at 80 ℃ for 48 hours under normal pressure, stripping from the glass substrate to obtain an aerogel film, and roasting at 350 ℃ for 4 hours to obtain the self-supporting high-moisture-permeability heat-insulating aerogel film.
The obtained self-supporting high-moisture-permeability heat-insulating aerogel thin film is 180 mu m thick and is a flat film, a hollow fiber film is formed by rolling, the heat conductivity coefficient of the hollow fiber film is 0.029W/(mK), the porosity is 87%, the strength is 1.4MPa, the exchange efficiency of water vapor is 70%, and the exchange efficiency is improved by 75% compared with that of the traditional solid composite film (40%).
Example 7
(1) Preparing a template: sequentially soaking a glass substrate in ethanol, acetone and deionized water, respectively ultrasonically washing for 30min, removing surface oil stains, filtering a solution of acrylamide/2-acrylamide-2-methylpropanesulfonic acid terpolymer (PAMS) with the concentration of 16wt.% by microporous filter paper with the aperture of 30-50 mu m, and coating the solution on the glass substrate with the coating thickness of 210 mu m to obtain a template for later use;
(2) hydrolysis of nanocellulose: uniformly dispersing 15g of nano-cellulose whiskers in 85mL of dimethylacetamide under the heating and stirring at 60 ℃, adding 17.2mL of methyltrimethoxysilane, 1.5mL of hydrochloric acid with the concentration of 0.1mol/L and 3.5mL of deionized water, adding acid, adjusting the pH value of the solution to 6, and hydrolyzing at 50 ℃ for 7 hours;
(3) preparing an aerogel film: after the hydrolysis is finished, standing for 24h, adding 0.3ml of 10mol/L concentrated ammonia water for gelation to enable the colloid viscosity to reach 10cP, coating the obtained gel on one side of the template with the PAMS by using a mechanical film coating machine to form an aerogel film with the thickness of 150 micrometers, quickly soaking the aerogel film in ethanol for 48h, replacing the ethanol for 3 times during the period, and taking out to obtain the template loaded with the aerogel film;
(4) and (3) carrying out aftertreatment on the aerogel film: the template loaded with the aerogel film is subjected to normal butane to replace ethanol in silica sol at the constant temperature of 60 ℃, and then the volume ratio of TMCS: n-hexane = 1: and (2) soaking the mixed solution of 12 for 48 hours for surface modification, drying at 80 ℃ for 48 hours under normal pressure, stripping from the glass substrate to obtain an aerogel film, and roasting at 350 ℃ for 4 hours to obtain the self-supporting high-moisture-permeability heat-insulating aerogel film.
The thickness of the obtained self-supporting high-moisture-permeability heat-insulating aerogel thin film is 300 mu m, the thin film is a flat film, the heat conductivity coefficient is 0.0289W/(mK), the porosity is 92%, the strength is 2.0MPa, the exchange efficiency of water vapor is 85%, and the heat-insulating aerogel thin film is improved by 112.5% compared with the traditional solid composite film (40%).
Example 8
(1) Preparing a template: sequentially soaking a glass substrate in ethanol, acetone and deionized water, respectively ultrasonically washing for 35min, removing surface oil stains, filtering a 20wt.% solution of acrylamide/2-acrylamido-2-methylpropanesulfonic acid terpolymer (PAMS) through microporous filter paper with the aperture of 30-50 mu m, coating the solution on the glass substrate, and obtaining a template with the coating thickness of 150 mu m for later use;
(2) hydrolysis of nanocellulose: uniformly dispersing 5g of nano-cellulose whiskers in 95mL of dimethylacetamide while heating and stirring at 40 ℃, then adding 22.4mL of silsesquioxane, 2mL of oxalic acid with the concentration of 0.5mol/L and 3.5mL of deionized water, adding acid, adjusting the pH of the solution to 25, and hydrolyzing at 80 ℃ for 12 hours;
(3) preparing an aerogel film: after the hydrolysis is finished, standing for 24h, adding 1ml of concentrated ammonia water with the concentration of 10mol/L for gelation to enable the colloid viscosity to reach 7cP, coating the obtained gel on one side of the template with the PAMS by using a mechanical film coating machine to form an aerogel film with the thickness of 200 micrometers, quickly soaking the aerogel film in a mixed solution of ethanol and ethyl orthosilicate (ethanol: ethyl orthosilicate = 1: 4 v/v) for 48h, changing the mixed solution for 3 times during the soaking period, and taking out to obtain the template loaded with the aerogel film;
(4) and (3) carrying out aftertreatment on the aerogel film: the template loaded with the aerogel film is subjected to n-butane to replace ethanol in silica sol at the constant temperature of 40 ℃, and then the volume ratio of TMCS: n-hexane = 1: 15 for 32 hours, drying at 80 ℃ under normal pressure for 48 hours, stripping from the glass substrate to obtain an aerogel film, and roasting at 350 ℃ for 4 hours to obtain the self-supporting high-moisture-permeability heat-insulating aerogel film.
The obtained self-supporting high-moisture-permeability heat-insulating aerogel thin film is 250 mu m thick, is a flat film, has the heat conductivity coefficient of 0.03W/(mK), the porosity of 83 percent, the strength of 1.8MPa and the exchange efficiency of water vapor of 95 percent, and is improved by 137.5 percent compared with the traditional solid composite film (40 percent).
Example 9
(1) Preparing a template: sequentially soaking a glass substrate in ethanol, acetone and deionized water, respectively ultrasonically washing for 20min, removing surface oil stains, filtering a solution of 10wt.% acrylamide/2-acrylamido-2-methylpropanesulfonic acid terpolymer (PAMS) through microporous filter paper with the aperture of 30-50 mu m, coating the solution on the glass substrate, and obtaining a template with the coating thickness of 250 mu m for later use;
(2) hydrolysis of nanocellulose: uniformly dispersing 12g of nano-cellulose whisker into 88mL of dimethylacetamide while heating and stirring at 40 ℃, then adding 27.2mL of silsesquioxane, 1mL of oxalic acid with the concentration of 0.8mol/L and 2mL of deionized water, adding acid, then adjusting the pH of the solution to 5, and hydrolyzing for 6h at 80 ℃;
(3) preparing an aerogel film: after the hydrolysis is finished, standing for 24h, adding 1.5ml of concentrated ammonia water with the concentration of 10mol/L for gelation to enable the colloid viscosity to reach 8cP, coating the obtained gel on the side, with the PAMS, of the template by using a mechanical film coating machine to form an aerogel film with the thickness of 300 micrometers, quickly soaking the aerogel film in a mixed solution (4: 1 v/v) of ethanol and ethyl orthosilicate for 72h, replacing the mixed solution for 3 times during the soaking, and taking out to obtain the template loaded with the aerogel film;
(4) and (3) carrying out aftertreatment on the aerogel film: the template loaded with the aerogel film is subjected to n-butane to replace ethanol in silica sol at the constant temperature of 40 ℃, and then the volume ratio of TMCS: n-hexane = 1: and (3) soaking the mixed solution of 10 for 48 hours for surface modification, drying at 80 ℃ for 72 hours under normal pressure, stripping from the glass substrate to obtain an aerogel film, and roasting at 350 ℃ for 4 hours to obtain the self-supporting high-moisture-permeability heat-insulating aerogel film.
The obtained self-supporting high-moisture-permeability heat-insulating aerogel thin film is 150 mu m in thickness, is a flat film, has the heat conductivity coefficient of 0.0295W/(mK), the porosity of 87 percent, the strength of 1.5MPa and the exchange efficiency of water vapor of 110 percent, and is improved by 175 percent compared with the traditional solid composite film (40 percent).
The self-supporting high moisture-permeable heat-insulating aerogel film can be used for realizing air dehumidification and seawater desalination, is of a three-dimensional porous net structure, has an extremely low heat conductivity coefficient, and integrates high strength, high moisture permeability, high selective permeability and heat insulation; tests show that under the same experimental conditions, the water vapor exchange rate is improved by 50-200% compared with that of the traditional solid composite membrane, and the heat conductivity coefficient is reduced by 50-90%; meanwhile, the self-supporting high-moisture-permeability heat-insulating aerogel film has the advantage of high porosity; the preparation method of the self-supporting high-moisture-permeability heat-insulating aerogel film is simple, easy to operate, low in equipment investment, high in porosity and good in film forming property.
Claims (10)
1. A preparation method of a self-supporting high-moisture-permeability heat-insulating aerogel film is characterized by comprising the following steps:
(1) cleaning the glass substrate, and removing oil stains on the surface; filtering the solution of the high molecular polymer by microporous filter paper, and coating the solution on a glass substrate to obtain a template for later use;
(2) uniformly dispersing the nano cellulose whiskers in an organic solvent under heating and stirring, and then adding a silicon source, acid and deionized water for hydrolysis;
(3) after the hydrolysis is finished, standing, adding gel liquid for gelation, coating the obtained gel on one side of the template with the high molecular polymer to form an aerogel film, quickly soaking the aerogel film in a solvent, and taking out the aerogel film to obtain the template loaded with the aerogel film;
(4) and (2) carrying out solvent exchange and surface modification on the template loaded with the aerogel film, drying, stripping from the glass substrate to obtain the aerogel film, and roasting at high temperature to obtain the self-supporting high-moisture-permeability heat-insulating aerogel film.
2. The preparation method of the self-supporting high moisture-permeable heat-insulating aerogel film according to claim 1, wherein in the step (1), the glass substrate is sequentially soaked in ethanol, acetone and deionized water for 20-40 min by ultrasonic wave respectively; the high molecular polymer comprises acrylamide/2-acrylamide-2-methylpropanesulfonic acid terpolymer; the mass concentration of the solution of the high molecular polymer is 10-20 wt.%; the pore size of the microporous filter paper is 30-50 mu m.
3. The preparation method of the self-supporting high moisture-permeable heat-insulating aerogel film according to claim 1, wherein in the step (2), the nano-cellulose whiskers are prepared by the following steps:
dissolving cellulose powder in concentrated sulfuric acid under heating and stirring, cooling to room temperature, and centrifugally washing with distilled water to obtain a non-stratified milky suspension; and dialyzing and separating the obtained milky suspension, and washing, freezing and drying the obtained crystal to obtain the nano cellulose whisker.
4. The preparation method of the self-supporting high moisture-permeable heat-insulating aerogel film according to claim 3, wherein the heating and stirring for dissolving the cellulose powder in the concentrated sulfuric acid under heating and stirring is performed at 60-80 ℃; the concentration of the concentrated sulfuric acid is 50-70 wt.%; the step of cooling to room temperature is to directly add distilled water for cooling; the dialysis is to put the milky suspension obtained by centrifugation into a cellulose dialysis bag and put the cellulose dialysis bag into deionized water for dialysis until the pH value of the dialysate reaches 7.0; the freeze drying is carried out at-30 to-50 ℃.
5. The method for preparing a self-supporting high moisture-permeable heat-insulating aerogel film according to claim 1, wherein in the step (2), the silicon source comprises one of methyl orthosilicate, ethyl orthosilicate, methyltrimethoxysilane, water glass, trimethylethoxysilane and silsesquioxane; according to different silicon sources, the added organic solvent is different: when the silicon source is methyl orthosilicate, the organic solvent is dimethyl sulfoxide; when the silicon source is tetraethoxysilane, the organic solvent is ethanol; when the silicon source is methyltrimethoxysilane, the organic solvent is tetrahydrofuran; when the silicon source is sodium silicate, the organic solvent is toluene; the silicon source is trimethyl ethoxy silane or silsesquioxane, and the organic solvent is dimethyl acetamide.
6. The preparation method of the self-supporting high moisture-permeable heat-insulating aerogel film according to claim 1, wherein in the step (2), the solid-to-liquid ratio of the nano cellulose whiskers to the organic solvent is 5-10: 80-100 g/mL; the mass ratio of the organic solvent to the silicon source is0.8-1.5: 0.3 to 0.6; the volume ratio of the organic solvent to the deionized water is 30-50: 2-4; the addition amount of the acid is 10 according to the molar ratio of hydrogen atoms in the acid to silicon atoms in the silicon source-5~10-3: 1-3, and the pH of the solution after the acid is added is 5-6.
7. The method for preparing the self-supporting high moisture-permeable heat-insulating aerogel film according to claim 1, wherein in the step (2), the heating and stirring are performed at 40-80 ℃; the hydrolysis temperature is 40-80 ℃, and the hydrolysis time is 6-12 h.
8. The preparation method of the self-supporting high moisture-permeable heat-insulating aerogel film as claimed in claim 1, wherein in the step (3), the standing time is 24-48 h; the gel liquid comprises more than one of ammonia water, ethanol, dimethyl sulfoxide and hexamethyldisilazane; adding gel liquid into the gel to make the viscosity of the gel reach 7-20 cP; the solvent comprises more than one of ethanol, ethyl orthosilicate and dimethyl sulfoxide; the soaking time is 24-72 h, and the solvent is replaced every 8-16 h.
9. The preparation method of the self-supporting high moisture-permeable heat-insulating aerogel film according to claim 1, wherein in the step (4), the solvent used for soaking in the step (3) is replaced by one of dimethyl sulfoxide, n-hexane, n-heptane and n-butane at a constant temperature of 40-60 ℃, and then the solution of trimethylchlorosilane is used for soaking for 24-48h for surface modification; the solvent of the solution of the trimethylchlorosilane is one of n-hexane, n-heptane and n-butane, wherein the volume ratio of the trimethylchlorosilane to the solvent is 1: 9-15; the drying is carried out at the temperature of 80-120 ℃ and under normal pressure for 24-48 h; the high-temperature roasting temperature is 350-450 ℃, and the time is 4-8 h.
10. A self-supporting high moisture-permeable heat-insulating aerogel film prepared by the preparation method of any one of claims 1 to 9, characterized in thatIs made of SiO2The self-supporting single-layer film with the porous framework structure has a heat conductivity coefficient of 0.02-0.03W/(mK) and a thickness of 150-300 mu m, and comprises two film types, namely a flat film and a hollow fiber film; the SiO2The porous skeleton structure is a three-dimensional network structure; the hollow fiber membrane is formed by rolling the flat membrane.
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| CN108816055B (en) * | 2018-07-04 | 2021-05-14 | 青岛科技大学 | Preparation method of biodegradable oil-water separation porous membrane |
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| CN114059737B (en) * | 2021-11-17 | 2023-06-02 | 瑞宇建设有限公司 | Construction process of curtain wall-imitating thermal insulation decorative external wall board |
| CN115364692B (en) * | 2022-08-12 | 2023-08-25 | 中国科学院上海高等研究院 | Air filtration composite membrane prepared based on cellulose nanofiber reinforced hydrogel conversion and preparation method thereof |
| CN115124758A (en) * | 2022-08-17 | 2022-09-30 | 大连海洋大学 | Preparation process of aerogel composite material |
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